関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Dichloromethane | HCID 6344 | — |
| 反応物 | 4-Methylanisole | HCID 7731 | — |
| 反応物 | Methane, dichloromethoxy- | HCID 21004 | — |
| 触媒 | Titanium Tetrachloride | HCID 24193 | — |
| 溶媒 | Water | HCID 962 | — |
| 生成物 | 2-Methoxy-5-methylbenzaldehyde | HCID 591398 | — |
反応手順
4-Methylanisole (12.2 g., 0.1 mole) in 300 ml. of methylene chloride was cooled to 0° C. Titanium tetrachloride (3.8 g., 0.2 mole) was added followed by the dropwise addition of 1,1-dichloromethyl methyl ether (13.8 g., 0.12 mole) over 3 minutes. After stirring for 30 minutes at 0° C., the reaction mixture was poured into 600 ml. of water. The aqueous phase was extracted with two further portions of methylene chloride. The combined organic phase/extracts was washed with brine, dried over anhydrous magnesium sulfate and evaporated to yield 2-methoxy-5-methylbenzaldehyde as an oil [15 g., 100%; ir (CH2Cl2) 1678, 1608, 1488 cm-1 ].
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US04399296 |
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| 出典データセット | uspto-grants-1983_08 |
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| ORD ID | ord-44924957485f4b0fa7614bf7cc871ae6 |
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| 出典メモ | uspto-grants-1983_08 |
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